CN1883729B - Method for processing rectified residue of ketene dimer - Google Patents
Method for processing rectified residue of ketene dimer Download PDFInfo
- Publication number
- CN1883729B CN1883729B CN2006100857960A CN200610085796A CN1883729B CN 1883729 B CN1883729 B CN 1883729B CN 2006100857960 A CN2006100857960 A CN 2006100857960A CN 200610085796 A CN200610085796 A CN 200610085796A CN 1883729 B CN1883729 B CN 1883729B
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- CN
- China
- Prior art keywords
- residue
- acetone
- ketene dimer
- temperature
- hydrolysis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000000034 method Methods 0.000 title claims abstract description 17
- WASQWSOJHCZDFK-UHFFFAOYSA-N diketene Chemical compound C=C1CC(=O)O1 WASQWSOJHCZDFK-UHFFFAOYSA-N 0.000 title claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 30
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000007062 hydrolysis Effects 0.000 claims description 11
- 238000006460 hydrolysis reaction Methods 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 239000003085 diluting agent Substances 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 238000003672 processing method Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- 235000021419 vinegar Nutrition 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000000446 fuel Substances 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- CCGKOQOJPYTBIH-UHFFFAOYSA-N ethenone Chemical compound C=C=O CCGKOQOJPYTBIH-UHFFFAOYSA-N 0.000 abstract 1
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- -1 Dichlorodiphenyl Acetate Chemical compound 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention disclose a method for recovering effective ingredient of residue and rectification treatment by ketene dimmer without pollution to environment. The method is characterized as: (1) using solvent to dilute residue (2) hydrolyzing diluted residue (3) separating and recovering acetone and acetic acid (4) facilitating polymerization or looping high polymer to obtain solid substance. The invention has a simple process. Valuable acetone and acetic acid in the residue can be indirectly recovered and obtained solid substance can be uses as industrial fuel, which solve the problem of residue pollution.
Description
Technical field
The present invention relates to the Dichlorodiphenyl Acetate pyrolysis method and produce the method that the rectification residue that produces in the ketene dimer process carries out environmental protection treatment.
Background technology
The acetic acid pyrolysis method is the main method of producing ketene dimer at present, the rectifying of the ketene dimer crude product process that is absolutely necessary wherein, producing about residue of about 10% in the distillation process is rectification residue, contain materials such as a certain amount of ketene dimer, aceticanhydride and ketene dimer high polymer in the rectification residue, residue viscosity is big and penetrating odor arranged, present most ketene dimer manufacturer all adopts the method for landfill or burning to handle, these two kinds of methods have not only caused pollution to environment, and have wasted ketene dimer and aceticanhydride valuable in the residue.
Summary of the invention
At the problems referred to above, the purpose of this invention is to provide the processing method of the ketene dimer rectification residue of effective ingredient in a kind of recyclable residue and environmentally safe.
For achieving the above object, the technical solution used in the present invention is: comprise dilution, hydrolysis, separation, four steps of curing:
(1) dilution: add diluent acetone in the residue of behind ketene dimer rectification, discharging, thereby be convenient to next step hydrolysis, and the volume ratio of diluent and residue is 1: 2～1: 5 with this viscosity that reduces residue.
(2) hydrolysis: distilled water is preheating to 50 ℃～60 ℃, ratio with volume ratio 1 ‰～5 ‰ adds sulfuric acid as catalyst, under stirring condition, drip the residue after diluting and control dropping temperature at 50 ℃～60 ℃, the carbon dioxide that produces in dropping process emptying after cooling off, it is complete to guarantee hydrolysis to be added dropwise to complete back insulation a period of time.Above chemical equation is as follows:
CH
2COCH
2CO+H
2O→CH
3COCH
3+CO
2
CH
3COOOCCH
3+H
2O——→2CH
3COOH
N in the three-step reaction equation≤4.
(3) separate: the rising temperature is to isolate the acetone in the hydrolyzate, keeping 70 ℃ waits not have till the obvious discharging, can obtain the acetone of content more than 95% this moment, material behind the removal acetone is continued to heat up with extraction acetic acid wherein, and the control temperature is not more than 150 ℃ of spirit of vinegars that finally can get about 45%.The acetone that is recovered to can be used as the diluent in the step (1), and the spirit of vinegar of acquisition can further be proposed dense use.
(4) solidify: the ratio with volume ratio 5%～10% adds NaOH as catalyst in leftover materials, treat to discharge while hot when temperature slowly rises to 160 ℃～200 ℃, can get solid-state atrament after the cooling.Can be after the solid-state atrament that obtains pulverized directly as industrial fuel.
The further technical scheme of the present invention is: being added dropwise to complete the back temperature retention time in the step (2), to be no less than 30 minutes complete to guarantee hydrolysis.
Advantage of the present invention is: (1) technology is simple, easy to operate.(2), valuable acetate and acetone in the residue have been reclaimed.(3), at last the solid matter that obtains can be done industrial fuel, has thoroughly solved the pollution problem of residue to environment.
The specific embodiment
Below in conjunction with embodiment technical solutions according to the invention are further described.
The operational instances step is as follows:
(1) dilution: acetone is reclaimed in the industry that adds 100mL in the 500mL two neck flasks that agitating device is housed, and opens and stirs the ketene dimer rectification residue that adds 300mL, fully stirs it is fully mixed.
(2) hydrolysis: the distilled water that in the 1000mL four neck flasks that stirring, measurement, condenser pipe and dropping liquid feeding device are housed, adds 200mL, ratio with volume ratio 3 ‰ adds 98% concentrated sulfuric acid, stir on the electric furnace and be preheating to 50～60 ℃, under stirring condition, drip the dilution of (1) preparation fully and control dropping temperature at 50～60 ℃, the carbon dioxide that produces in dropping process emptying after cooling off, it is complete to guarantee hydrolysis to be incubated 30 minutes after being added dropwise to complete.
(3) separate: after above-mentioned insulation is finished, acetone in the rising temperature distilling material, insulation distillation 1 hour and temperature are controlled at 65 ℃ and can get the water white liquid acetone of 170mL, analyzing content is 97%, switch the acetic acid in the discharging bottle leftover materials to be recycled, the rising temperature reaches will have acetic acid to steam about 120 ℃, stop heating and be incubated 30 minutes getting colourless transparent liquid 300mL when temperature reaches 130 ℃, and the acetic acid content of analyzing wherein is 45.8%.
(4) solidify: get the solid sodium hydroxide of 5g, grind to form powdery and under stirring condition, add, treat after the adding that temperature warms up when slowly rising to 180 ℃ to discharge fast, after the cooling the black solid material, be weighed as 101g.Can be after the black solid material pulverized directly as industrial fuel.
Claims (2)
1. the processing method of ketene dimer rectification residue, described ketene dimer rectification residue are that the acetic acid pyrolysis method is produced the rectification residue that produces in the ketene dimer process, it is characterized in that: comprise dilution, hydrolysis, separation, four steps of curing:
(1) dilution: add diluent acetone in the residue of behind ketene dimer rectification, discharging, and the volume ratio of diluent and residue is 1: 2～1: 5.
(2) hydrolysis: distilled water is preheating to 50～60 ℃, ratio with volume ratio 1 ‰～5 ‰ adds sulfuric acid as catalyst, under stirring condition, drip the residue after diluting and control dropping temperature at 50～60 ℃, the carbon dioxide that produces in dropping process emptying after cooling off, it is complete to guarantee hydrolysis to be added dropwise to complete back insulation a period of time;
(3) separate: the rising temperature is to isolate the acetone in the hydrolyzate, keeping 70 ℃ waits not have till the obvious discharging, can obtain the acetone of content more than 95% this moment, material behind the removal acetone is continued to heat up with extraction acetic acid wherein, and the control temperature is not more than 150 ℃ of spirit of vinegars that finally can get about 45%;
(4) solidify: the ratio with volume ratio 5%～10% adds NaOH as catalyst in leftover materials, treat to discharge while hot when temperature slowly rises to 160 ℃～200 ℃, can get solid-state atrament after the cooling.
2. processing method according to claim 1 is characterized in that: being added dropwise to complete the back temperature retention time in the step (2), to be no less than 30 minutes complete to guarantee hydrolysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100857960A CN1883729B (en) | 2006-06-30 | 2006-06-30 | Method for processing rectified residue of ketene dimer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100857960A CN1883729B (en) | 2006-06-30 | 2006-06-30 | Method for processing rectified residue of ketene dimer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1883729A CN1883729A (en) | 2006-12-27 |
| CN1883729B true CN1883729B (en) | 2010-06-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2006100857960A Active CN1883729B (en) | 2006-06-30 | 2006-06-30 | Method for processing rectified residue of ketene dimer |
Country Status (1)
| Country | Link |
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| CN (1) | CN1883729B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337869B (en) * | 2008-08-01 | 2011-09-28 | 江苏天成生化制品有限公司 | Processing process for ketene dimer rectification residue |
| CN102295544B (en) * | 2010-06-22 | 2015-04-08 | 上海华谊工程技术有限公司 | Method for treating raw distillation raffinate of isopropenyl acetate |
| CN101886011B (en) * | 2010-07-07 | 2012-12-19 | 苏州浩波科技股份有限公司 | Processing method for wastes after recovery processing diketene rectification |
| CN103113186B (en) * | 2012-11-11 | 2014-12-31 | 安徽金禾实业股份有限公司 | Treating method and treating device for ketene dimer production residues |
| CN110128350A (en) * | 2019-07-01 | 2019-08-16 | 山东汇海医药化工有限公司 | A method of improving 5-acetoacetamido benzimidazolone quality |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU789502A1 (en) * | 1978-01-30 | 1980-12-23 | Рошальский Ордена Трудового Красного Знамени Химический Комбинат | Method of extracting acetone and acetic acid from still residue in acetic anhydride production |
-
2006
- 2006-06-30 CN CN2006100857960A patent/CN1883729B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU789502A1 (en) * | 1978-01-30 | 1980-12-23 | Рошальский Ордена Трудового Красного Знамени Химический Комбинат | Method of extracting acetone and acetic acid from still residue in acetic anhydride production |
Non-Patent Citations (3)
| Title |
|---|
| 钟曾玲.双乙烯酮生产中醋酸回收工艺流程优化.天然气化工27.2002,2726-28. * |
| 陈建文.双乙烯酮残渣的综合利用研究.广东化工33 1.2006,33(1),52-53. |
| 陈建文.双乙烯酮残渣的综合利用研究.广东化工33 1.2006,33(1),52-53. * |
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| Publication number | Publication date |
|---|---|
| CN1883729A (en) | 2006-12-27 |
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Address after: 215633, Nansha, Jiangsu Province, Zhangjiagang Town, three gold road Patentee after: SUZHOU HOPE TECHNOLOGY CO.,LTD. Address before: 215633, Nansha, Jiangsu Province, Zhangjiagang Town, three gold road Patentee before: Zhangjiagang Haobo Chemical Co.,Ltd. |
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Denomination of invention: Method for processing rectified residue of ketene dimer Effective date of registration: 20150209 Granted publication date: 20100630 Pledgee: Bank of Communications Ltd. Zhangjiagang branch Pledgor: SUZHOU HOPE TECHNOLOGY CO.,LTD. Registration number: 2015990000121 |
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Date of cancellation: 20220822 Granted publication date: 20100630 Pledgee: Bank of Communications Ltd. Zhangjiagang branch Pledgor: SUZHOU HOPE TECHNOLOGY CO.,LTD. Registration number: 2015990000121 |
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Effective date of registration: 20221024 Address after: 226009 No. 968, Jiangshan Road, Nantong Economic and Technological Development Zone, Nantong City, Jiangsu Province Patentee after: NANTONG HONGXIN CHEMICAL Co.,Ltd. Address before: 215633, Nansha, Jiangsu Province, Zhangjiagang Town, three gold road Patentee before: SUZHOU HOPE TECHNOLOGY CO.,LTD. |